不同产地保健食品原料中总砷及无机砷含量检测

李亚贤; 田怀香; 于海燕; 陆智

doi:10.13386/j.issn1002-0306.2021120117

不同产地保健食品原料中总砷及无机砷含量检测

doi: 10.13386/j.issn1002-0306.2021120117

1.
无限极（中国）有限公司，广东广州 510665
2.
上海应用技术大学香料香精化妆品学部，上海 201418

基金项目: 国家重点研发计划项目（2018YFC1602106）。

详细信息

作者简介:
李亚贤（1985−），女，硕士，工程师，研究方向：食品安全，E-mail：Yaxian.Li@infinitus-int.com

通讯作者:
陆智（1981−），男，硕士，工程师，研究方向：食品安全，E-mail：Chris.Lu@infinitus-int.com。

中图分类号: O657.6；TS218
计量
- 文章访问数: 111
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- PDF下载量: 24
- 被引次数: 0
出版历程
- 收稿日期: 2021-12-13
- 网络出版日期: 2022-04-28
- 刊出日期: 2022-06-15

Detection of Total Arsenic and Inorganic Arsenic Content in Health Food Raw Materials from Different Habitats

1.
Infinitus (China) Co. Ltd., Guangzhou 510665, China
2.
Department of Perfume and Aroma Technology, Shanghai Institute of Technology, Shanghai 201418, China

摘要

摘要: 为考察保健食品原料中砷污染情况，确保保健食品的质量安全，采用电感耦合等离子体质谱（ICP-MS）和高效液相色谱-电感耦合等离子体质谱（HPLC/ICP-MS）法对来自16个产地14种保健食品原料中总砷和无机砷含量进行测定。结果表明，总砷和无机砷浓度与信号强度在0~100 μg/L范围内呈良好的线性关系，样品检测结果的相对标准偏差（RSD）在0.00~2.52%之间，精密度良好。所检测保健食品原料中，总砷含量在（0.0004~0.3900）mg/kg之间，未超出保健食品限量标准；无机砷的含量在（0.0003~0.1962）mg/kg之间。河北金银花的总砷及无机砷含量最高；吉林的人参、新疆的大枣、云南的核桃肉、安徽的白芍、山西的山萸肉及福建的猴头菇等6种原料的砷含量较低，其中人参、大枣、核桃肉的总砷含量相同，且为最低，为0.0004 mg/kg，无机砷含量亦相同，为0.0003 mg/kg。本研究给出了多种保健食品原料不同产地的砷残留数据，扩充了保健食品原料砷含量数据库，为砷污染风险评估提供了重要参考。
- 保健食品原料 /
- 总砷 /
- 无机砷 /
- ICP-MS /
- HPLC/ICP-MS
Abstract: To investigate the arsenic pollution in health food raw materials and to ensure the quality and safety of health food, the contents of total arsenic and inorganic arsenic in 14 kinds of health food raw materials from 16 habitats were determined by inductively coupled plasma-mass spectrometry (ICP-MS) and high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC/ICP-MS), respectively. The relationship between arsenic concentration and signal intensity is linear with R² higer than 0.9999 in range of 0~100 μg/L. The relative standard deviation (RSD) of detecting results of health food raw materials were from 0.00% to 2.52%, and the precision was satisfactory. The total arsenic content was between (0.0004~0.3900) mg/kg, which did not exceed the health food limit standard. The content of the inorganic arsenic was (0.0003~0.1962) mg/kg. Among them, total arsenic and inorganic arsenic content of Hebei honeysuckle was the highest, the contents of arsenic in ginseng from Jilin, jujube from Xinjiang, walnut from Yunnan, white peony root from Anhui, cornus officinalis from Shanxi and Hericium erinaceus from Fujian were low. The total arsenic contents of ginseng, jujube and walnut meat were the same and the lowest, 0.0004 mg/kg, and the inorganic arsenic contents were also the same, 0.0003 mg/kg. The data of arsenic residues in a variety of health food raw materials were given, which expanded the arsenic content database of health food raw materials and would provide an important reference for arsenic pollution risk assessment.

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表 1 微波消解仪升温程序

Table 1. Heating program of microwave digestion instrument

步骤	功率（W）	升温时间（min）	控制温度（℃）	保持时间（min）	控制压力（Bar）
1	1200	5	120	6	10
2	1200	5	160	6	20
3	1200	5	190	20	30

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表 2 五种样品ICP-MS与AFS两种方法总砷含量结果对比

Table 2. Comparison of the results of total arsenic content of five samples by ICP-MS and AFS

保健食品原料	产地	ICP-MS		AFS
保健食品原料	产地	含量（mg/kg）	RSD（%）	含量（mg/kg）	RSD（%）
茯苓	安徽安庆	0.0068	0.05	未检出	−
茯苓	云南大理	0.0261	0.02	未检出	−
黄芪	内蒙古	0.0886	0.06	未检出	−
	青海	0.1155	0.04	未检出	−
	甘肃	0.0689	0.03	未检出	−

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表 3 砷在基质中的添加回收率和变异系数

Table 3. Recovery rate and coefficient of variation of arsenic added to the matrix

添加量（μg）	样品号	实际检出量（μg）	回收率（%）	平均回收率（%）	变异系数（%）
0.0010	1	0.00095	95.00	90.00	3.51
	2	0.00090	90.00
	3	0.00090	90.00
	4	0.00090	90.00
	5	0.00085	85.00
	6	0.00090	90.00
0.0030	1	0.00285	95.00	100.00	4.94
	2	0.00315	105.00
	3	0.00315	105.00
	4	0.00305	101.70
	5	0.00280	93.33
	6	0.00300	100.00
0.0100	1	0.00940	94.00	101.00	5.87
	2	0.00985	98.50
	3	0.00980	98.00
	4	0.01085	108.50
	5	0.00975	97.50
	6	0.01075	107.50

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表 4 保健食品原料样品中的总砷含量

Table 4. Total arsenic content in health food raw materials samples

保健食品原料名	产地	含量（mg/kg）	保健食品原料名	产地	含量（mg/kg）
金针菇	浙江江山	0.0470±0.0032^c	核桃肉	云南	0.0004±0.0000^a
	福建	0.0310±0.0085^bc	黄精	福建	0.1370±0.0058^f
	浙江常山	0.0280±0.0067^b	生地黄	河南	0.2830±0.0252^h
金银花	山东	0.0770±0.0139^d	猴头菇	福建	0.0110±0.0046^a
	河南	0.2970±0.0208^hi	葛根	安徽	0.0210±0.0036^b
	河北	0.3900±0.0200^j	玄参	浙江	0.1800±0.0100^g
巴戟天	广东肇庆	0.2900±0.0100^h		河南	0.1300±0.0100^f
巴戟天	广东云浮	0.3100±0.0200ⁱ		湖北	0.1370±0.0058^f
木耳	福建	0.1644±0.0013^g	人参	吉林	0.0004±0.0000^a
木耳	浙江	0.1078±0.0013^e	山萸肉	山西	0.0020±0.0020^a
白芍	安徽	0.0021±0.0017^a	大枣	新疆	0.0004±0.0000^a
注：上标不同小写字母表示数据存在显著差异（P<0.05）；表6同。

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表 5 无机砷在基质中的添加回收率和变异系数

Table 5. Recovery rate and coefficient of variation of inorganic arsenic added to the matrix

添加量（μg）	样品号	信号强度		实际检出量（μg）	回收率（%）	平均回收率（%）	变异系数（%）
添加量（μg）	样品号	As（III）	As（V）	实际检出量（μg）	回收率（%）	平均回收率（%）	变异系数（%）
0.100	1	76010.17	161621.88	0.0951	95.09	95.00	0.54
	2	76555.35	160698.42	0.0952	95.21
	3	75143.21	160390.60	0.0940	94.05
	4	75789.45	162356.88	0.0952	95.16
	5	76393.13	162168.42	0.0956	95.55
	6	76018.15	160698.42	0.0948	94.80
0.300	1	202597.09	465791.36	0.2871	95.71	94.90	0.69
	2	202908.23	458340.87	0.2850	95.00
	3	204628.86	459019.33	0.2865	95.50
	4	201817.88	456745.24	0.2837	94.55
	5	202200.84	451681.92	0.2823	94.11
	6	200637.12	456877.16	0.2828	94.27
1.000	1	658320.60	1533428.17	0.9698	96.98	97.00	0.10
	2	657618.52	1534031.24	0.9694	96.94
	3	658921.63	1532674.32	0.9700	97.00
	4	657094.63	1535413.29	0.9695	96.95
	5	657440.35	1531499.58	0.9685	96.85
	6	657903.08	1535897.00	0.9702	97.02

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表 6 保健食品原料样品中无机砷含量

Table 6. Inorganic arsenic content in health food raw materials samples

保健食品原料名	产地	三价砷（mg/kg）	五价砷（mg/kg）	无机砷（mg/kg）	无机砷/总砷（%）
金针菇	浙江江山	0.0280	0.0066	0.0346±0.0016^d	73.62
	福建	0.0230	0.0319	0.0308±0.0026^c	99.35
	浙江常山	0.0170	0.0403	0.0256±0.0052^c	91.43
金银花	山东	0.0150	0.0078	0.0228±0.0030^b	29.61
	河南	0.0790	0.0171	0.0961±0.0038^h	32.36
	河北	0.0050	0.1912	0.1962±0.0026^m	50.31
巴戟天	肇庆	0.0250	0.1098	0.1348±0.0059^j	46.48
巴戟天	云浮	0.0000	0.1736	0.1736±0.0013^l	56.00
木耳	福建	0.0250	0.0442	0.0691±0.0020^e	42.03
木耳	浙江	0.0059	0.0614	0.0673±0.0036^e	62.43
白芍	安徽	0.0018	0.0000	0.0018±0.0001^a	85.71
猴头菇	福建	0.0000	0.0009	0.0009±0.0004^a	8.18
葛根	安徽	0.0037	0.0017	0.0054±0.0007^a	25.71
玄参	浙江	0.0103	0.0981	0.1084±0.0031ⁱ	60.22
	河南	0.0074	0.0670	0.0744±0.0015^f	57.23
	湖北	0.0072	0.0833	0.0905±0.0047^g	66.06
山萸肉	山西	0.0000	0.0008	0.0008±0.0002^a	40.00
人参	吉林	0.0000	0.0000	0.0003±0.0002^a	75.00
大枣	新疆	0.0000	0.0000	0.0003±0.0002^a	75.00
核桃肉	云南	0.0000	0.0000	0.0003±0.0000^a	75.00
黄精	福建	0.0124	0.0190	0.0314±0.0013^d	22.92
生地黄	河南	0.0167	0.1337	0.1504±0.0054^k	53.14

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